CN101293632A - Method for converting H2S into hydrogen gas with photocatalysis decomposition - Google Patents

Method for converting H2S into hydrogen gas with photocatalysis decomposition Download PDF

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CN101293632A
CN101293632A CNA2007101067691A CN200710106769A CN101293632A CN 101293632 A CN101293632 A CN 101293632A CN A2007101067691 A CNA2007101067691 A CN A2007101067691A CN 200710106769 A CN200710106769 A CN 200710106769A CN 101293632 A CN101293632 A CN 101293632A
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hydrogen
reaction
organic solvent
decomposition
photocatalysis decomposition
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李�灿
马贵军
鄢洪建
吴国鹏
宗旭
栾国有
雷志斌
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

The invention relates to a method for transforming H2S into hydrogen and sulfur in a way of photocatalysis decomposition. By taking an alcohol amine organic solvent as the absorbent of hydrogen sulfide gas and adding in a photocatalyst of semiconductor powder with a formula being Mx-Cd1-yZnyS, the decomposition reaction of H2S under light condition is carried out. The method of the invention realizes the process of directly decomposing H2S to produce a product H2 and an element S, thus providing an approach for simultaneously recycling H2 and simple substance S from the H2S by utilizing a photocatalysis method.

Description

A kind of photocatalysis Decomposition H 2S is converted into the method for hydrogen and sulphur
Technical field
The invention belongs to photochemical catalysis and produce the energy field of hydrogen and the environmental area that sulfurous gas is eliminated in degraded, relate in particular to a kind of photocatalysis Decomposition H 2S is converted into the method for hydrogen and sulphur.
Background technology
Along with the exhaustion day by day of petroleum-based energy and the deterioration year by year of world environments, energy development of new, cleaning more and more is subjected to the attention of national governments and scientists, to all progressively expansion of research and development of sun power, wind energy, tidal energy, nuclear energy and Hydrogen Energy.Wherein, Hydrogen Energy becomes the emphasis of exploitation as the energy of a kind of high-energy-density, high-level efficiency, cleaning, and in addition, hydrogen also is one of most important material in the chemical industry, is used for synthetic ammonia, synthesizing methanol, petroleum refining etc. in a large number.The hydrogen major part is that raw material is produced with the fossil oil in the world at present, and small portion comes from brine electrolysis and other.Along with the increase of hydrogen demand amount and the reduction of fossil oil reserves, develop new, high-level efficiency, hydrogen producing technology has very important significance for the energy security and the economic Sustainable development of country cheaply.
The hydrogen sulfide waste gas that discharges in Chemical Manufacture and oil, the natural gas processing process is a kind of toxic gas of contaminate environment, at present, industrial most employing Kraus process is handled the hydrogen sulfide recovery sulphur, be that hydrogen sulfide part incomplete oxidation and permutoid reaction are converted into sulphur and water, but this cause Hydrogen Energy to waste greatly.So, if can invent a kind of decomposing H 2The method of S-not only simple and easy to do but also can from hydrogen sulfide, reclaim sulphur and hydrogen-very big application prospect will be arranged simultaneously.
Sun power is extremely abundant and the very cheap energy, utilizes light-catalysed method decomposing H 2S gas all has report in a lot of patents.
One) U.S. Philps Petroleum Company once applied for two Chinese patent: CN86102715A and CN86102648A respectively in 1986.In patent, the contriver adopts alkaline liquid as H 2The lyosorption of S carries out H 2The photolysis of S and photocatalysis Decomposition, but there is following point in these two inventions:
1, light-catalyzed reaction activity is low, and when reaction conditions is in the 100 gram solution, under the situation that 1.0～1.3 gram catalyzer exist, filtering the sub-efficient of its maximum amount at 350 nanometer passbands is 5%, and the sub-efficient of its maximum amount has only 1.1% under 400 nanometer passbands filter.
2, in the product of decomposition reaction, only related to H 2Detection, to H 2S among the S 2-The final processing of light-catalyzed reaction is not considered.
3, H 2The lyosorption of S is the aqueous solution of basic cpd or the pyrrolidone solution of having dissolved basic cpd, this means and will additionally add basic cpd, also brings difficulty for the aftertreatment of product.
Two) this grade of Lanzhou Inst. of Chemical Physics, Chinese Academy of Sciences's Japanese plum people once applied for a patent CN1068546A, had reported with ZnFe 2O 4Be photocatalyst, make the method for hydrogen sulfide and low-carbon alcohol dehydrogenation under the illumination.But there is following problem equally:
1, reactive behavior is low, and under 750 watts of xenon lamps shone, the product hydrogen activity of 25 milligrams of catalyzer was 0.67 milliliter.
2, only related to the detection of hydrogen, not to H 2S among the S 2-Handle.
3, need to add NaOH and absorb H 2S generates NaS, and this has not only consumed NaOH, also makes troubles for the aftertreatment of product.
In sum, research ubiquity in the past two problems: the one, the utilization of luminous energy is mostly concentrated on wavelength less than the ultraviolet region below the 420nm; Also having a problem is to H 2The decomposition of S mostly is to realize as sacrificing reagent by the aqueous solution of alkalescence, because H 2O has participated in H in photocatalysis oxidation reaction 2The oxidation of S, its final product are the oxysalt of hydrogen and sulfur oxide or sulfur-bearing, and elementary sulfur is not separated out with the form of elemental sulfur, and this has not only caused the waste of sulphur but also for aftertreatment brings difficulty, has become at present and hindered the photocatalytic method decomposing H 2One of bottleneck of S industrial application.
Summary of the invention
In order to make photocatalysis Decomposition H 2The recovery of hydrogen and elemental sulfur is accomplished in the reaction of S simultaneously, the object of the present invention is to provide a kind of photocatalysis Decomposition H 2S is converted into the method for hydrogen and sulphur.
For achieving the above object, adopt anhydrous or aqueous alcamine compound as H among the present invention 2The lyosorption of S has been avoided alkaline assistants such as additive decrementation alkali metal hydroxide, has shown good H 2The S receptivity adopts M x-Cd 1-yZn yS series sulfide semiconductor, shows good photochemical catalysis and produces hydrogen activity in this reaction system as photocatalyst applications, adopts 0.025g CdS catalyzer, and the quantum yield at the 420nm place reaches more than 30%, is the highest level of existing patent report; The more important thing is S in patent in the past 2-Be oxidized to complicated rhodanine salt, make H 2S is converted into the more unmanageable pollutent of another kind by a kind of pollutent, and adopts the alcamines reaction system in the present invention, S 2-Ion is turned to elemental sulfur and polysulfide by the photocatalytic-oxidation of selectivity, has made things convenient for the aftertreatment of product.Its primary process is:
H 2S absorbs: H 2S+EA → H 2S-EA
H 2S photocatalysis Decomposition: H 2S-EA → H 2+ S+EA
Total reaction: H 2S → H 2+ S
EA represents the alcamines lyosorption
In detail, photocatalysis Decomposition H provided by the invention 2S is converted into the method for hydrogen and sulphur, adopts the absorption agent of alcamines organic solvent as hydrogen sulfide, and adding expression formula again is M x-Cd 1-yZn yThe semiconductor powder photocatalyst of S carries out H under illumination 2The decomposition reaction of S; Expression formula M x-Cd 1-yZn yAmong the S:
M is one or more among Fe, Co, Ni, Cu, Ag, Hg, Pb, In, Ga, the Bi;
X is the amount of substance mark, 0≤x≤1;
Y is the amount of substance mark, 0≤y≤1.
Described method.Wherein be connected to simultaneously on the carbochain in the molecular formula of alcamines organic solvent in amino and hydroxyl or the whole solvent and contain amino group and oh group.
Described method, wherein the water content of alcamines organic solvent is counted 0-90% by volume.
Described method, wherein the alcamines organic solvent is one or more in thanomin, diethanolamine, trolamine, diisopropanolamine (DIPA), the methyldiethanolamine.
Described method, wherein the semiconductor powder photocatalyst is CdS.
Described method, wherein the surface of semiconductor powder photocatalyst has supported promotor, and its expression formula of promotor is M I+ M IIS, wherein: M IBe among precious metal Ru, Rh, Pd, Ir, Pt, the Au one or more; M IIBe among Pd, Mo, the W one or more.
Method provided by the invention can realize H 2S directly decomposes product H 2With the process of element S, this is for utilizing photocatalytic method from H 2Reclaim H among the S simultaneously 2And simple substance S provides a kind of approach.
Description of drawings
Accompanying drawing 1 is different Pt loading time catalyzing and decomposing H 2The reactive behavior figure of S.
Accompanying drawing 2 is photocatalysis Decomposition H under the differing temps 2The product hydrogen activity figure of S.
Accompanying drawing 3 is photocatalysis Decomposition H under the different catalysts consumption 2The reactive behavior figure of S.
Accompanying drawing 4 different H 2Photocatalysis Decomposition H under the S concentration 2The reactive behavior figure of S.
Embodiment
The present invention is achieved by the following technical solutions:
Adopt the absorption agent of anhydrous or aqueous alcamines organic solvent, under agitation continuous absorption H as hydrogen sulfide 2S gas absorbs photocatalyst to be dispersed in after finishing and has absorbed H 2In the solvent of S, place photo catalysis reactor to carry out photocatalysis Decomposition H solvent again 2The reaction of S.
Be used for estimating photocatalysis Decomposition H in the present invention 2The reactor of S is a round tube type top illuminaton reactor, and 7 centimetres of cylinder interior diameters are high 7 centimetres, adopts Pyrex glass to make, and reactor top adds a watercooling jacket, is used for the elimination infrared light, catalyzer with absorbed H 2The organic solvent of S places reactor, adopt magnetic stirring apparatus to stir, system is found time then to shine with xenon lamp, wavelength region by adding spectral filter and optical filtering water jacket control incident light at 420nm between the 1000nm, the temperature of reaction of system is controlled by external watercooling jacket, and the hydrogen of generation carries out online detection by gas-chromatography.
CdS adopts Hydrothermal Preparation in the embodiments of the invention, and the original position photoreduction met hod is adopted in supporting of semiconductor surface precious metal, adopts the xenon lamp simulated solar irradiation of CERAMAX.
Embodiments of the invention only are used for illustrating the present invention, should not think to the restricted property of the present invention.For example, be to adopt the alcamines organic solvent of anhydrous or moisture (being that water content is counted 0-90% by volume) among the embodiment as H 2The absorption agent of S, but any anhydrous or aqueous liquid medium all is fit to the present invention, as long as this liquid medium can absorb H 2S or after adding another kind of liquid medium to H 2S has receptivity, all can use the present invention.
Embodiments of the invention are as follows:
Embodiment 1:
This example is used for illustrating H 2S is from absorbing the whole process of decomposition.
Get the 100ml organic solvent and place brown bottle, adopt magnetic stirring apparatus to stir, feed H continuously 2S gas, pilot-gas flow velocity about 60ml/min, absorb finish after with gained H 2The absorption liquid of S changes in the reactor of photochemical catalysis evaluating apparatus, add a certain amount of semiconductor powder photocatalyst that has supported precious metal, stirring makes its homodisperse, system is found time afterwards to adopt xenon lamp to carry out illumination, control certain reaction temperature, and by adding spectral filter and optical filtering water jacket, between the 1000nm, the hydrogen of generation carries out online detection by gas-chromatography to the wavelength region of control incident light at 420nm.
Embodiment 2:
This example adopts the flow process of embodiment 1 to estimate, and is used for illustrating adopting different organic lyosorptions to carry out photocatalysis Decomposition H 2The difference of the product hydrogen activity of S, its reaction result such as table 1:
Table 1:
Lyosorption Produce hydrogen activity (mmol/h)
Thanomin 0.8
Diethanolamine 1.4
Trolamine 0.8
Diethylamide 0.4
In above-mentioned reaction, the H that absorbs in the 100ml solvent 2The amount of S is controlled at 30 ± 3mmol, and temperature of reaction is controlled between 15 to 25 degrees centigrade, and catalyzer is the CdS powder, and the precious metal that the surface supports is Pt 0.2wt%, and catalyst levels is 0.025g, and xenon lamp intensity is 300W.
Reaction result shows that in selected organic solvent, diethanolamine has shown best photochemical catalysis and produced hydrogen activity, so in the reaction test below, unless show especially, the solvent that is adopted is all diethanolamine.
Embodiment 3:
This example adopts the flow process of embodiment 1 to estimate, and is used for illustrating adopting the light source of varying strength to carry out photocatalysis Decomposition H 2The difference of the product hydrogen activity of S, its reaction result such as table 2:
Table 2:
The intensity of light source Produce hydrogen activity (mmol/h)
300W 2.0
150W 0.8
In above-mentioned reaction, the H that absorbs in the 100ml diethanolamine 2The amount of S is controlled at 10 ± 1mmol, and temperature of reaction is controlled between 50 to 60 degrees centigrade, and catalyzer is the CdS powder, and the precious metal that the surface supports is Pt 0.2wt%, and catalyst levels is 0.025g
Reaction result shows, adopts the xenon lamp of its reactive behavior of xenon lamp of 300W apparently higher than 150W, so in the reaction test below, unless show especially, the light source that is adopted is all the xenon lamp of 300W.
Embodiment 4:
This example adopts the flow process of embodiment 1 to estimate, and is used for illustrating the precious metals pt that supports different amounts on the CdS semiconductor light-catalyst, carries out photocatalysis Decomposition H 2The difference of the product hydrogen activity of S, its reaction result is seen Fig. 1.
In above-mentioned reaction, the H that absorbs in the 100ml diethanolamine 2The amount of S is controlled at 10 ± 1mmol, and temperature of reaction is controlled between 50 to 60 degrees centigrade, and catalyzer is the CdS powder, and the precious metal that the surface supports is Pt, and catalyst levels is 0.025g.
Embodiment 5:
This example adopts the flow process of embodiment 1 to estimate, and is used for illustrating adopting different photocatalysts to carry out photocatalysis Decomposition H 2The difference of the product hydrogen activity of S, its reaction result such as table 3:
Table 3
Photocatalyst Consumption (gram) Promotor Loading (wt%) Produce hydrogen activity (mmol/h)
Cu 0.04Zn 0.96S 0.10 Do not have 0 0.09
(CuIn) 0.045Zn 0.91S 0.10 Rh 2S 3 0.05 0.09
Bi 2S 3 0.10 Do not have 0 0.17
Cu 0.01Cd 0.01Zn 0.98S 0.10 Do not have 0 0.01
Cu 0.02Cd 0.1Zn 0.88S 0.10 Do not have 0 0.01
Cd 0.88Zn 0.12S 0.025 Pt 0.2 0.13
Cd 0.85Zn 0.15S 0.025 Pt 0.2 0.04
Cd 0.79Zn 0.21S 0.025 Pt 0.2 0.03
Cd 0.33Zn 0.67S 0.025 Pt 0.2 0.01
CdS 0.025 Pt 0.2 1.4
In above-mentioned reaction, the H that absorbs in the 100ml diethanolamine 2The amount of S is controlled at 30 ± 3mmol, and temperature of reaction is controlled between 15 to 25 degrees centigrade.
Embodiment 6:
This example adopts the flow process of embodiment 1 to estimate, and is used for illustrating that CdS supports different noble metal promoted agent and carries out photocatalysis Decomposition H 2The product hydrogen activity of S, its reaction result such as table 4:
Table 4:
Precious metal Loading (wt%) Produce hydrogen activity (mmol/h)
Do not have 0 0.2
Pt 0.2 1.4
Ru 0.2 0.9
Rh 0.2 0.9
Pd 0.2 0.5
Au 0.2 0.2
PdS 0.2 1.1
RhS 0.2 1.3
Pt-Rh 0.2-0.1 1.6
Pt-Rh 0.2-0.2 1.6
Pt-RhS 0.2-0.2 1.0
Pt-PdS 0.2-0.2 1.5
In above-mentioned reaction, the H that absorbs in the 100ml diethanolamine 2The amount of S is controlled at 30 ± 3mmol, and temperature of reaction is controlled between 15 to 25 degrees centigrade, and catalyzer is the CdS powder, and catalyst levels is 0.025g.
Embodiment 7:
This example adopts the flow process of embodiment 1 to estimate, and is used for illustrating CdS photocatalyst light-catalyzed reaction decomposing H after 5 hours under differing temps 2Total hydrogen output of S, its reaction result is seen Fig. 2.
In above-mentioned reaction, the H that absorbs in the 100ml diethanolamine 2The amount of S is controlled at 30 ± 3mmol, and catalyzer is the CdS powder, and the precious metal that the surface supports is Pt 0.2wt%, and catalyst levels is 0.025g.
The result shows, at photocatalysis Decomposition H 2In the reaction of S, temperature is influential to the product hydrogen activity of reaction, shows that tentatively control reaction temperature shows the highest hydrogen output at 50 degrees centigrade.
Embodiment 8:
This example adopts the flow process of embodiment 1 to estimate, and is used for illustrating photocatalysis Decomposition H under different CdS photocatalyst consumptions 2The product hydrogen activity of S, its reaction result is seen Fig. 3.
In above-mentioned reaction, the H that absorbs in the 100ml diethanolamine 2The amount of S is controlled at 30 ± 3mmol, and temperature of reaction is controlled between 15 to 25 degrees centigrade, and catalyzer is the CdS powder, and the precious metal that the surface supports is Pt 0.2wt%.
Embodiment 9:
This example adopts the flow process of embodiment 1 to estimate, and is used for illustrating that the CdS photocatalyst is at different H 2Photocatalysis Decomposition H under the S concentration 2The product hydrogen activity of S, its reaction result is seen Fig. 4.
In above-mentioned reaction, the consumption of diethanolamine solvent is 100ml, and temperature of reaction is controlled between 15 to 25 degrees centigrade, and catalyzer is the CdS powder, and the precious metal that the surface supports is Pt 0.2wt%, and catalyst levels is 0.025g.
Embodiment 10:
This example adopts the flow process of embodiment 1 to estimate, and is used for illustrating the mixed solvent time catalyzing and decomposing H that employing is different 2The product hydrogen activity of S, its reaction result such as table 4:
Table 4:
Mixed solvent (volume ratio) Produce hydrogen activity (mmol/h)
Diethanolamine 90%+ water 10% 1.9
Diethanolamine 70%+ thanomin 30% 1.0
Diethanolamine 70%+ trolamine 30% 1.3
Diethanolamine 70%+ ethylamine 30% 1.1
Diethanolamine 70%+ ethanol 30% 1.9
Diethanolamine 70%+ ethylene glycol 30% 1.5
In above-mentioned reaction, the H that absorbs in the 100ml mixed solvent 2The amount of S is controlled at 30 ± 3mmol, and temperature of reaction is controlled between 15 to 25 degrees centigrade, and catalyzer is the CdS powder, and the precious metal that the surface supports is Pt 0.2wt%, and catalyst levels is 0.025g.

Claims (6)

1, a kind of photocatalysis Decomposition H 2S is converted into the method for hydrogen and sulphur, adopts the absorption agent of alcamines organic solvent as hydrogen sulfide, and adding expression formula again is M x-Cd 1-yZn yThe semiconductor powder photocatalyst of S carries out H under illumination 2The decomposition reaction of S; Expression formula M x-Cd 1-yZn yAmong the S:
M is one or more among Fe, Co, Ni, Cu, Ag, Hg, Pb, In, Ga, the Bi;
X is the amount of substance mark, 0≤x≤1;
Y is the amount of substance mark, 0≤y≤1.
2, the described method of claim 1.Wherein, be connected to amino in the molecular formula of described alcamines organic solvent on the carbochain simultaneously and hydroxyl or whole solvent in contain amino group and oh group.
3, the described method of claim 2, wherein, the water content of described alcamines organic solvent is counted 0-90% by volume.
4, claim 2 or 3 described methods, wherein, described alcamines organic solvent is one or more in thanomin, diethanolamine, trolamine, diisopropanolamine (DIPA), the methyldiethanolamine.
5, the described method of claim 1, wherein, described semiconductor powder photocatalyst is CdS.
6, the described method of claim 1, wherein, the surface of described semiconductor powder photocatalyst has supported promotor, and its expression formula of promotor is M I+ M IIS, wherein: M IBe among precious metal Ru, Rh, Pd, Ir, Pt, the Au one or more; M IIBe among Pd, Mo, the W one or more.
CNA2007101067691A 2007-04-25 2007-06-20 Method for converting H2S into hydrogen gas with photocatalysis decomposition Pending CN101293632A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101927173B (en) * 2010-02-01 2011-12-21 黑龙江省科学院石油化学研究院 Photocatalyst for preparing hydrogen and sulphur by decomposing hydrogen sulfide and preparation method thereof
CN102773057A (en) * 2012-08-09 2012-11-14 西安交通大学 Photocatalytic decomposition reactor of hydrogen sulfide based on fluidized bed technology and hydrogen producing device for photocatalytic decomposition reactor of hydrogen sulfide
CN102814186A (en) * 2012-09-07 2012-12-12 中国科学院长春应用化学研究所 Photolytic hydrogen production catalyst and preparation method thereof
CN104368369A (en) * 2014-10-09 2015-02-25 济南大学 Preparation method of silver phosphate-cadmium sulfide composite visible light photocatalyst
CN105603450A (en) * 2014-11-13 2016-05-25 中国科学院大连化学物理研究所 Method for preparing hydrogen and sulfur through photoelectrocatalysis-chemical ring reaction coupling decomposition of hydrogen sulfide
US9579639B2 (en) 2013-09-05 2017-02-28 Saudi Arabian Oil Company Tethered transition metals promoted photocatalytic system for efficient hydrogen evolutions
CN109420514A (en) * 2017-08-21 2019-03-05 中国科学院上海硅酸盐研究所 A kind of nickel single-site graphite phase carbon nitride base optic catalytic material and its preparation method and application

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101927173B (en) * 2010-02-01 2011-12-21 黑龙江省科学院石油化学研究院 Photocatalyst for preparing hydrogen and sulphur by decomposing hydrogen sulfide and preparation method thereof
CN102773057A (en) * 2012-08-09 2012-11-14 西安交通大学 Photocatalytic decomposition reactor of hydrogen sulfide based on fluidized bed technology and hydrogen producing device for photocatalytic decomposition reactor of hydrogen sulfide
CN102773057B (en) * 2012-08-09 2015-08-26 西安交通大学 A kind of photocatalysis Decomposition hydrogen sulfide reactor based on fluidization and device for producing hydrogen thereof
CN102814186A (en) * 2012-09-07 2012-12-12 中国科学院长春应用化学研究所 Photolytic hydrogen production catalyst and preparation method thereof
US9579639B2 (en) 2013-09-05 2017-02-28 Saudi Arabian Oil Company Tethered transition metals promoted photocatalytic system for efficient hydrogen evolutions
CN104368369A (en) * 2014-10-09 2015-02-25 济南大学 Preparation method of silver phosphate-cadmium sulfide composite visible light photocatalyst
CN105603450A (en) * 2014-11-13 2016-05-25 中国科学院大连化学物理研究所 Method for preparing hydrogen and sulfur through photoelectrocatalysis-chemical ring reaction coupling decomposition of hydrogen sulfide
CN109420514A (en) * 2017-08-21 2019-03-05 中国科学院上海硅酸盐研究所 A kind of nickel single-site graphite phase carbon nitride base optic catalytic material and its preparation method and application

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